CN109514017B - Vacuum diffusion welding process for hard alloy and steel - Google Patents

Vacuum diffusion welding process for hard alloy and steel Download PDF

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CN109514017B
CN109514017B CN201811433385.5A CN201811433385A CN109514017B CN 109514017 B CN109514017 B CN 109514017B CN 201811433385 A CN201811433385 A CN 201811433385A CN 109514017 B CN109514017 B CN 109514017B
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temperature
furnace
hard alloy
steel
welding
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CN109514017A (en
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孙小傅
孙锦民
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Zigong Zhongxing Wear Resistant New Materials Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00Soldering, e.g. brazing, or unsoldering
    • B23K1/008Soldering within a furnace
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00Soldering, e.g. brazing, or unsoldering
    • B23K1/20Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00Soldering, e.g. brazing, or unsoldering
    • B23K1/20Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
    • B23K1/206Cleaning
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31Coating with metals
    • C23C18/32Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
    • C23C18/34Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
    • C23C18/36Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions

Abstract

A vacuum diffusion welding process of hard alloy and steel comprises the following steps: pre-welding treatment; plating Ni on the pretreated hard alloy; carrying out recrystallization annealing on the brazing filler metal; vacuum diffusion welding, which is to weld dissimilar metals of hard alloy and steel by adopting vacuum diffusion welding and realize diffusion welding by strictly controlling technological parameters such as temperature, connection pressure, connection time and the like.

Description

Vacuum diffusion welding process for hard alloy and steel
Technical Field
The invention relates to the field of dissimilar material welding, in particular to a vacuum diffusion welding process of hard alloy and steel.
Background
The hard alloy has excellent performances of high hardness, high wear resistance and the like, so the hard alloy is widely applied to the industrial fields of machining, geological exploration, mining and the like, but the price is high, the steel has higher strength and good toughness, is easy to weld and wear, and if the steel and the hard alloy are compounded, the steel and the hard alloy are well combined by a certain process method to form the WC welding nail made of the hard alloy-steel composite wear-resistant material.
Because the hard alloy and the steel belong to the connection of dissimilar materials, the hard alloy and the steel need to be combined to form a composite welding nail by a specific process method, and then the WC welding nail is welded with the alloy steel by an arc stud welding method, so that the WC welding nail not only has the toughness as the alloy steel, but also has the high hardness and the high wear resistance as the hard alloy, and the price is lower than that of the hard alloy; however, the thermal expansion coefficient difference between the hard alloy WC and the alloy steel is large, so that the welded joint generates large thermal stress in the cooling process, and the heterogeneous connection between the hard alloy WC and the alloy steel faces great difficulty.
The hard alloy and the steel have great differences in thermal physical properties, linear expansion coefficients and the like, and due to the great differences, a eutectic structure of compounds is easy to appear in the middle, so that a brittle phase and great stress are easy to generate at a joint when the hard alloy and the steel are welded, welding cracks are easy to occur, the performance of the joint is reduced, and the welding of the hard alloy and the hard alloy involves the following problems in terms of weldability.
The melting point, the heat conductivity, the linear expansion coefficient and the mechanical property of the hard alloy and the steel are greatly different, the low-melting-point base metal is melted firstly during welding, the high-melting-point base metal is difficult to melt under the heating condition, and the joint part can generate great thermal stress during welding to increase the crack tendency. The welding seam is easy to generate hot cracks when the steel and the hard alloy are welded, which is related to low melting point eutectic generated at a joint, grain boundary segregation and larger linear expansion coefficient difference, the grain boundary segregation of the low melting point eutectic in the welding seam weakens the connection between grains, and larger welding stress is easy to cause, so that the hot cracks are generated.
Disclosure of Invention
The invention overcomes the defects of large welding line expansion difference of dissimilar materials and brittle phase generation among metals in the prior art, and provides a vacuum diffusion welding process of hard alloy and steel, which comprises the following steps:
pre-welding treatment: roughly grinding a spreading test surface and a brazing surface of hard alloy and steel on a diamond grinding machine, then coating diamond grinding paste on an iron casting block, and placing the spreading surface and the brazing surface on cast iron for grinding until the surfaces are bright; roughly grinding 45 steel on a grinding machine, and then polishing a spreading test surface and a brazing surface by using metallographic abrasive paper; polishing the brazing filler metal and the iron sheet by using metallographic abrasive paper to be bright, and removing an oxide layer;
soaking all polished materials in acetone for 5-10 minutes during brazing, scrubbing, taking out and drying;
plating Ni on the pretreated hard alloy, wherein the plating process conditions are as follows: the alkali washing temperature is 60 ℃, and the alkali washing time is 10-15 min; after alkali washing, carrying out acid washing in hydrochloric acid for 10-15 s; the plating temperature is 80 ℃;
carrying out recrystallization annealing on the brazing filler metal;
vacuum diffusion welding: firstly, placing the processed hard alloy and steel into a vacuum furnace, vacuumizing the furnace to 14Pa, applying 10MPa of pre-pressure when the vacuum degree reaches 14Pa, starting to heat up to 200 ℃ at the average speed of 22.5 ℃/min, and then starting to heat up to 500 ℃ at the speed of 25 ℃/min; the heating temperature is kept between 400 and 500 ℃ during diffusion welding, the heat preservation time is 60-180min, the welding pressure is 0-10Mpa, and after the welding is finished, the furnace is cooled to be below 100 ℃.
As a further limitation of the invention, the formula of the electroless nickel plating solution is as follows: 28g/L of nickel sulfate, 19g/L of sodium acetate, 17g/L of sodium citrate, 29g/L of sodium hypophosphite, 6-7 drops of thiourea and 30 drops of lactic acid, and adjusting the pH value to 4.5-5; the alkaline washing liquid comprises the following formula: 20g/L of sodium hydroxide, 35g/L of trisodium phosphate, 25g/L of sodium carbonate and 2.5g/L of sodium silicate.
As a further limitation of the present invention, the recrystallization annealing treatment specifically includes: firstly, a box type resistance heating furnace is subjected to empty furnace heating and heat preservation for 60min to homogenize the furnace temperature, then the box type resistance heating furnace is closed, the furnace door is quickly opened to send brazing filler metal into the furnace, the furnace door is quickly closed, the box type resistance heating furnace is opened to continue heating, heat preservation treatment is carried out when the temperature reaches the annealing temperature, natural cooling is carried out after the heat preservation treatment, after annealing, No. 01 and No. 03 abrasive paper are used for rough grinding, No. 05 and No. 07 fine grinding are respectively used for fine grinding, and then A1203 polishing solution is used for polishing velvet until the surface is smooth and has no scratch.
As a further limitation of the invention, the brazing filler metal is CuMnNi, CuMnTi and iron sheet.
Selection of temperature: as the research on the diffusion welding of the dissimilar metals of the hard alloy and the 45 steel is not reported, the welding temperature can be selected only according to an empirical formula, namely the temperature required by the common diffusion welding is 0.6-0.8 Tm, Tm is the melting temperature of the metal, and the temperature range is 400-500 ℃ considering that the temperature is too low, the diffusion effect is poor, the temperature is too high, the crystal grains grow seriously and the joint strength is reduced.
Selection of pressure: the welding surface is very uneven, therefore, pressure is required to be applied in the welding process to enable the microcosmic convex part of the welding surface to generate plastic deformation and activate atoms in an interface area and eliminate interface holes, so that the welding surface is close to the distance within which the interatomic bonding force acts to complete interatomic bonding on the welding surface, the required welding pressure depends on the hardness, yield strength, toughness and plasticity, linear expansion coefficient and the like of the material, the 7075 aluminum alloy has good plasticity, and has a larger difference with the linear expansion coefficient of the magnesium alloy, so the selected pressure is not suitable to be too large, otherwise, the deformation is serious, larger welding residual stress is generated, and the joint strength is greatly reduced; in consideration of ensuring the close contact of the welding surfaces and avoiding the residual stress of welding, the invention adopts the welding pressure of 0-10 MPa.
The beneficial effects of the invention are:
according to the recrystallization theory, a heating furnace is utilized to carry out recrystallization annealing treatment on the brazing filler metal, so that the matrix structure of the brazing filler metal is refined, and a good base material is provided for diffusion welding; when the hard alloy and the steel are welded, the physical and chemical properties of the hard alloy and the steel are different and influenced, so that the weldability of the hard alloy and the steel is poor, a large amount of intermetallic compounds with high brittleness and high hardness can be generated on a joint interface, and the performance of a welding joint is seriously influenced; by plating Ni on the hard alloy, the generation of intermetallic compounds is avoided or reduced, and the types and distribution states of the intermetallic compounds generated at joints are improved, so that the strength of the joints is improved; the vacuum diffusion welding is adopted to weld dissimilar metals of hard alloy and steel, and the diffusion welding is realized by strictly controlling technological parameters such as temperature, connecting pressure, connecting time and the like.
Drawings
FIG. 1 is a view showing the structure of the brazing material of the present invention.
Detailed Description
The invention will be further elucidated with reference to the following specific examples; it should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the claimed invention; further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teachings of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example one
A vacuum diffusion welding process of hard alloy and steel.
Pre-welding treatment: roughly grinding a spreading test surface and a brazing surface of hard alloy and steel on a diamond grinding machine, coating diamond grinding paste on an iron casting block, finally placing the spreading surface and the brazing surface on cast iron for grinding until the surfaces are bright, roughly grinding 45 steel on a grinding machine, then grinding the spreading test surface and the brazing surface to be bright by using metallographic abrasive paper, cutting the brazing filler metal CuMnNi into sheets, wherein the sizes of the brazing filler metal CuMnNi are slightly larger than the brazing surface so as to ensure that the brazing filler metal quantity is enough to fill up brazing gaps, grinding the brazing filler metal and the iron sheets to be bright by using the metallographic abrasive paper, and removing an oxide layer;
during brazing, all polished materials are soaked in acetone for 5-10 minutes, scrubbed, taken out and dried to prevent the sample from being polluted again, and vacuum diffusion brazing needs to be carried out as soon as possible;
The pretreated hard alloy is plated with Ni, and the formula of the plating solution for chemical nickel plating is as follows: 28g/L of nickel sulfate, 19g/L of sodium acetate, 17g/L of sodium citrate, 29g/L of sodium hypophosphite, 6-7 drops of thiourea and 30 drops of lactic acid, and adjusting the pH value to 4.5-5;
the alkaline washing liquid comprises the following formula: 20g/L of sodium hydroxide, 35g/L of trisodium phosphate, 25g/L of sodium carbonate and 2.5g/L of sodium silicate;
the plating process conditions are as follows: the alkali washing temperature is 60 ℃, and the alkali washing time is 10-15 min; after alkali washing, carrying out acid washing in hydrochloric acid for 10-15 s; the plating temperature is 80 ℃;
and (3) carrying out recrystallization annealing on the brazing filler metal: calculating and determining the lowest recrystallization temperature of the brazing filler metal according to an empirical formula, firstly closing a switch in a box type resistance heating furnace to raise the furnace temperature to the crystallization temperature, keeping the temperature for 60min after the temperature reaches the crystallization temperature, homogenizing the furnace temperature, then turning off the resistance heating furnace, quickly opening a furnace door to convey the brazing filler metal into the furnace, quickly closing the furnace door, continuing heating by closing the switch, starting heat preservation when the temperature reaches the annealing temperature, naturally cooling after heat preservation, coarsely grinding with No. 01 and No. 03 abrasive paper, finely grinding with No. 05 and No. 07 respectively after annealing, and then polishing on velvet by using A1203 polishing solution until the surface is smooth and has no scratch;
Vacuum diffusion welding: in the test process, firstly, the processed hard alloy and steel are placed in a vacuum furnace, the hard alloy, the steel and brazing filler metal are assembled, a furnace door is closed, the furnace is vacuumized to 14Pa, parameters such as annealing temperature, heat preservation time, heating speed and the like are set on a controller, when the vacuum degree reaches 14Pa, pre-pressure of 10MPa is applied, the temperature starts to rise to a preset temperature at the speed of 22.5 ℃/min on average, when the temperature rises to 200 ℃, the pressure is gradually increased due to the self expansion of a welding material, and diffusion welding parameters are as follows: heating at 450 deg.C, holding for 100min, and welding under 5Mpa, and cooling to below 100 deg.C to prevent oxidation of welded joint at high temperature.
Shear strength test: firstly, processing a diffusion welding joint into a sample with the thickness of 10mm multiplied by 20mm, assembling the diffusion welding sample on a special clamp by adopting a DNS200 type micro-control electronic universal test press and a special clamp, and testing the shear strength of the diffusion welding joint on a universal test machine, wherein the loading speed is 1 mm/min.
Before the shearing test, the outer surface of the sample is ground flat to measure the shearing area and ensure the shearing precision, and then the shearing test is carried out on a test press, and the shearing strength of the brazed joint is 50.12KN/mm 2(ii) a And (3) hardness testing: firstly, grinding a welding sample into two surfaces with high parallelism and certain smoothness by using water sand paper, and continuously grinding, polishing and corroding the surface with the hardness to be measured according to the requirements of a metallographic sample; then, an HVS-1000A Vickers microhardness instrument is adopted to measure microhardness of different positions of the welding seam diffusion layer, and the hardness of the joint is 102 HV.
Example two
Pretreatment in welding: roughly grinding a spreading test surface and a brazing surface of hard alloy and steel on a diamond grinding machine, then coating diamond grinding paste on an iron casting block, and finally placing the spreading surface and the brazing surface on cast iron to grind until the surfaces are bright; roughly grinding 45 steel on a grinding machine, and then polishing a spreading test surface and a brazing surface by using metallographic abrasive paper; the brazing filler metal iron sheets are cut into sheets, the sizes of the brazing filler metal iron sheets are slightly larger than the brazing surface, so that the brazing filler metal amount is enough to fill up brazing gaps, the brazing filler metal and the iron sheets are polished to be bright by using metallographic abrasive paper, and an oxide layer is removed;
during brazing, all polished materials are soaked in acetone for 5-10 minutes, scrubbed, taken out and dried to prevent the sample from being polluted again, and vacuum diffusion brazing needs to be carried out as soon as possible;
plating Ni on the pretreated hard alloy, wherein the plating solution formula of the chemical nickel plating is as follows: 28g/L of nickel sulfate, 19g/L of sodium acetate, 17g/L of sodium citrate, 29g/L of sodium hypophosphite, 6-7 drops of thiourea and 30 drops of lactic acid, and adjusting the pH value to 4.5-5;
The alkaline washing liquid comprises the following formula: 20g/L of sodium hydroxide, 35g/L of trisodium phosphate, 25g/L of sodium carbonate and 2.5g/L of sodium silicate;
the plating process conditions are as follows: the alkali washing temperature is 60 ℃, and the alkali washing time is 10-15 min; after alkali washing, carrying out acid washing in hydrochloric acid for 10-15 s; the plating temperature is 80 ℃;
and (3) carrying out recrystallization annealing on the brazing filler metal: calculating and determining the lowest recrystallization temperature of the brazing filler metal according to an empirical formula, firstly closing a switch in a box type resistance heating furnace, raising the furnace temperature to an annealing temperature, keeping the temperature for 60min after the temperature reaches the annealing temperature, homogenizing the furnace temperature, then turning off the resistance heating furnace, quickly opening a furnace door, feeding the brazing filler metal into the furnace, quickly closing the furnace door, continuing heating by closing the switch, timing and keeping the temperature when the temperature reaches the annealing temperature, turning off the switch after the test heat preservation time, taking out the brazing filler metal after the furnace is cooled to the room temperature, coarsely grinding with No. 01 and No. 03 abrasive paper, finely grinding No. 05 and No. 07 respectively after annealing, and then polishing on velvet by using A1203 polishing liquid until the surface is smooth and has no scratch;
vacuum diffusion welding: in the test process, firstly, the processed hard alloy, steel and brazing filler metal are placed into a vacuum furnace, the hard alloy, the steel and the brazing filler metal are assembled, a furnace door is closed, the inside of the furnace is vacuumized to 14Pa, and parameters such as annealing temperature, heat preservation time, heating speed and the like are set on a controller; when the vacuum degree reaches 14Pa, applying 10MPa of pre-pressure, starting to heat to a preset temperature at the average speed of 22.5 ℃/min, and gradually increasing the pressure due to the self expansion of a welding material when the temperature is raised to 200 ℃, wherein the diffusion welding parameters are as follows: heating at 400 deg.C, holding for 60min, and welding under 10Mpa, and cooling to below 100 deg.C to prevent oxidation of welded joint at high temperature.
And (3) shear strength test: firstly, processing a diffusion welding joint into a sample of 10mm multiplied by 20mm, adopting a DNS200 type micro-control electronic universal test press and a special clamp, assembling the diffusion welding sample on the special clamp, testing the shear strength of the diffusion welding joint on the universal test machine, and setting the loading speed to be 1 mm/min.
Before the shear test, the outer surface of the sample is ground flat to measure the shear area and ensure the shear accuracy, and then the shear test is carried out on a test press.
The shear strength of the brazed joint is 55.34KN/mm2(ii) a And (3) testing hardness: firstly, grinding a welding sample into two surfaces with high parallelism and certain smoothness by using water sand paper, and continuously grinding, polishing and corroding the surface with the hardness to be measured according to the requirements of a metallographic sample; then, performing microhardness measurement on different positions of the welding seam diffusion layer by adopting an HVS-1000A Vickers microhardness instrument; the hardness of the joint was 122 HV.
EXAMPLE III
Pretreatment in welding: roughly grinding a spreading test surface and a brazing surface of hard alloy and steel on a diamond grinding machine, then coating diamond grinding paste on an iron casting block, and finally placing the spreading surface and the brazing surface on cast iron to grind until the surfaces are bright; roughly grinding 45 steel on a grinding machine, and then polishing a spreading test surface and a brazing surface by using metallographic abrasive paper; the brazing filler metal CuMnTi is cut into sheets, the size of each brazing filler metal CuMnTi is slightly larger than the brazing surface so as to ensure that the brazing filler metal quantity is enough to fill up brazing gaps, the brazing filler metal and iron sheets are polished to be bright by metallographic abrasive paper, and an oxide layer is removed;
During brazing, all polished materials are soaked in acetone for 5-10 minutes, scrubbed, taken out and dried to prevent the sample from being polluted again, and vacuum diffusion brazing needs to be carried out as soon as possible;
the pretreated hard alloy is plated with Ni, and the formula of the plating solution for chemical nickel plating is as follows: 28g/L of nickel sulfate, 19g/L of sodium acetate, 17g/L of sodium citrate, 29g/L of sodium hypophosphite, 6-7 drops of thiourea and 30 drops of lactic acid, and adjusting the pH value to 4.5-5;
the alkaline washing liquid comprises the following formula: 20g/L of sodium hydroxide, 35g/L of trisodium phosphate, 25g/L of sodium carbonate and 2.5g/L of sodium silicate;
the plating process conditions are as follows: the alkali washing temperature is 60 ℃, and the alkali washing time is 10-15 min; after alkali washing, carrying out acid washing in hydrochloric acid for 10-15 s; the plating temperature is 80 ℃;
and (3) carrying out recrystallization annealing on the brazing filler metal: calculating and determining the lowest recrystallization temperature of the brazing filler metal according to an empirical formula, firstly closing a switch in a box type resistance heating furnace, raising the furnace temperature to the annealing temperature, keeping the temperature for 60min after the temperature reaches the annealing temperature, homogenizing the furnace temperature, then turning off the resistance heating furnace, quickly opening a furnace door, feeding the brazing filler metal into the furnace, quickly closing the furnace door, continuing heating by closing the switch, timing and keeping the temperature when the temperature reaches the annealing temperature, turning off the switch after the test heat preservation time, taking out a sample after the furnace is cooled to the room temperature, coarsely grinding with No. 01 and No. 03 abrasive paper, finely grinding No. 05 and No. 07 respectively after annealing, and then polishing on velvet by using A1203 polishing liquid until the surface is smooth and has no scratch;
Vacuum diffusion welding: firstly, placing processed hard alloy, steel and brazing filler metal into a vacuum furnace, assembling the hard alloy, the steel and the brazing filler metal, closing a furnace door, vacuumizing the furnace to 14Pa, setting parameters such as annealing temperature, heat preservation time, heating speed and the like on a controller, applying 10MPa of pre-pressure after the vacuum degree reaches 14Pa, starting heating to a preset temperature at the average speed of 22.5 ℃/min, and gradually increasing the pressure due to the self expansion of a welding material when the temperature is increased to 200 ℃;
the diffusion welding parameters are: heating at 400 deg.C for 60min, maintaining at 10Mpa, and cooling to below 100 deg.C to prevent oxidation of welded joint at high temperature.
And (3) shear strength test: firstly, processing a diffusion welding joint into a sample with the thickness of 10mm multiplied by 20mm, assembling the diffusion welding sample on a special clamp by adopting a DNS200 type micro-control electronic universal test press and a special clamp, and testing the shear strength of the diffusion welding joint on a universal test machine at the loading speed of 1 mm/min.
Before the shear test, the outer surface of the sample was ground flat to measure the shear area and to ensure the shear accuracy, and then the shear test was performed on a test press.
The shear strength of the brazed joint is 55.67KN/mm2(ii) a And (3) testing hardness: firstly, grinding a welding sample into two surfaces with high parallelism and certain smoothness by using water sand paper; continuously grinding, polishing and corroding the surface with the hardness to be measured according to the requirements of the metallographic specimen; then, performing microhardness measurement on different positions of the welding seam diffusion layer by adopting an HVS-1000A Vickers microhardness instrument; the hardness of the joint was 125 HV.
Example four
Pretreatment in welding: roughly grinding a spreading test surface and a brazing surface of hard alloy and steel on a diamond grinding machine, then coating diamond grinding paste on an iron casting block, and finally placing the spreading surface and the brazing surface on cast iron to grind until the surfaces are bright; roughly grinding 45 steel on a grinding machine, and then polishing a spreading test surface and a brazing surface by using metallographic abrasive paper; the brazing filler metal CuMnNi is cut into sheets, the size of each sheet is slightly larger than the brazing surface so as to ensure that the brazing filler metal amount is enough to fill up brazing gaps, the brazing filler metal and iron sheets are polished by metallographic abrasive paper to be bright, and an oxide layer is removed;
during brazing, all polished materials are soaked in acetone for 5-10 minutes, scrubbed, taken out and dried to prevent the sample from being polluted again, and vacuum diffusion brazing needs to be carried out as soon as possible;
The pretreated hard alloy is plated with Ni, and the formula of the plating solution for chemical nickel plating is as follows: 28g/L of nickel sulfate, 19g/L of sodium acetate, 17g/L of sodium citrate, 29g/L of sodium hypophosphite, 6-7 drops of thiourea and 30 drops of lactic acid, and adjusting the pH value to 4.5-5;
the alkaline washing liquid comprises the following formula: 20g/L of sodium hydroxide, 35g/L of trisodium phosphate, 25g/L of sodium carbonate and 2.5g/L of sodium silicate;
the plating process conditions are as follows: the alkali washing temperature is 60 ℃, and the alkali washing time is 10-15 min; after alkali washing, carrying out acid washing in hydrochloric acid for 10-15 s; the plating temperature is 80 ℃;
and (3) carrying out recrystallization annealing on the brazing filler metal: calculating and determining the lowest recrystallization temperature of the brazing filler metal according to an empirical formula, firstly closing a switch in a box type resistance heating furnace, raising the furnace temperature to an annealing temperature, keeping the temperature for 60min after the temperature reaches the annealing temperature, homogenizing the furnace temperature, then turning off the resistance heating furnace, quickly opening a furnace door, feeding the brazing filler metal into the furnace, quickly closing the furnace door, continuing heating by closing the switch, timing and keeping the temperature when the temperature reaches the annealing temperature, turning off the switch after the test heat preservation time, taking out the brazing filler metal after the furnace is cooled to the room temperature, coarsely grinding with No. 01 and No. 03 abrasive paper, finely grinding No. 05 and No. 07 respectively after annealing, and then polishing on velvet by using A1203 polishing liquid until the surface is smooth and has no scratch;
Vacuum diffusion welding: in the test process, firstly, the processed hard alloy and steel are put into a vacuum furnace, the hard alloy, the steel and the brazing filler metal are assembled, a furnace door is closed, the inside of the furnace is vacuumized to 14Pa, and parameters such as annealing temperature, heat preservation time, heating speed and the like are set on a controller; when the vacuum degree reaches 14Pa, applying 10MPa of pre-pressure, starting to heat to a preset temperature at the speed of 22.5 ℃/min on average, and gradually increasing the pressure due to the self expansion of the welding material when the temperature is raised to 200 ℃.
The diffusion welding parameters were: heating at 500 deg.C for 100min, and welding under 10Mpa, and cooling the sample to below 100 deg.C to prevent oxidation of the welded joint at high temperature;
shear strength test: firstly, processing a diffusion welding joint into a sample with the thickness of 10mm multiplied by 20mm, assembling the diffusion welding sample on a special clamp by adopting a DNS200 type micro-control electronic universal test press and a special clamp, and testing the shear strength of the diffusion welding joint on a universal test machine, wherein the loading speed is 1 mm/min.
Before the shear test, the outer surface of the sample was ground flat to measure the shear area and to ensure the shear accuracy, and then the shear test was performed on a test press.
The shear strength of the brazed joint was 57KN/mm2(ii) a And (3) hardness testing: firstly, grinding a welding sample into two surfaces with high parallelism and certain smoothness by using water sand paper; continue to pressGrinding, polishing and corroding the surface with the hardness to be measured according to the requirements of a metallographic sample; then, performing microhardness measurement on different positions of the welding seam diffusion layer by adopting an HVS-1000A Vickers microhardness instrument; the hardness of the joint was 104 HV.
EXAMPLE five
Pretreatment in welding: roughly grinding a spreading test surface and a brazing surface of hard alloy and steel on a diamond grinding machine, then coating diamond grinding paste on an iron casting block, and finally placing the spreading surface and the brazing surface on cast iron to grind until the surfaces are bright; roughly grinding 45 steel on a grinding machine, and then polishing a spreading test surface and a brazing surface by using metallographic abrasive paper; the brazing filler metal iron sheet is cut into sheets, and the sizes of the brazing filler metal iron sheets are slightly larger than the brazing surface, so that the brazing filler metal is enough to fill a brazing gap; polishing the brazing filler metal and the iron sheet by using metallographic abrasive paper to be bright, and removing an oxide layer;
during brazing, all polished materials are soaked in acetone for 5-10 minutes, scrubbed, taken out and dried to prevent the sample from being polluted again, and vacuum diffusion brazing needs to be carried out as soon as possible;
The pretreated hard alloy is plated with Ni, and the formula of the plating solution for chemical nickel plating is as follows: 28g/L of nickel sulfate, 19g/L of sodium acetate, 17g/L of sodium citrate, 29g/L of sodium hypophosphite, 6-7 drops of thiourea and 30 drops of lactic acid, and adjusting the pH value to 4.5-5;
the alkaline washing liquid comprises the following formula: 20g/L of sodium hydroxide, 35g/L of trisodium phosphate, 25g/L of sodium carbonate and 2.5g/L of sodium silicate;
the plating process conditions are as follows: the alkali washing temperature is 60 ℃, and the alkali washing time is 10-15 min; after alkali washing, acid washing is carried out in hydrochloric acid, and the acid washing time is 10-15 s; the plating temperature is 80 ℃;
and (3) carrying out recrystallization annealing on the brazing filler metal: the lowest recrystallization temperature of the brazing filler metal is calculated and determined according to an empirical formula, a switch is closed in a box type resistance heating furnace at first, the furnace temperature is raised to the annealing temperature, the temperature is kept for 60min after the temperature is raised, the furnace temperature is homogenized, then the resistance heating furnace is turned off, a furnace door is rapidly opened, the brazing filler metal is conveyed into the furnace, the furnace door is rapidly closed, the switch is closed for continuous heating, the temperature is kept when the temperature reaches the annealing temperature, the switch is turned off after the test heat preservation time, the brazing filler metal is taken out after the furnace is cooled to the room temperature, after annealing, No. 01 and No. 03 abrasive papers are respectively used for rough grinding, No. 05 and No. 07 fine grinding, and then A1203 polishing liquid is used for polishing treatment on velvet until the surface is smooth and has no scratch.
Vacuum diffusion welding: in the test process, firstly, the processed hard alloy and steel are put into a vacuum furnace, the hard alloy, the steel and the brazing filler metal are assembled, a furnace door is closed, the furnace is vacuumized to 14Pa, and parameters such as annealing temperature, heat preservation time, heating speed and the like are set on a controller; when the vacuum degree reaches 14Pa, applying 10MPa of pre-pressure, starting to heat to a preset temperature at the average speed of 22.5 ℃/min, and gradually increasing the pressure due to the self expansion of the welding material when the temperature is raised to 200 ℃;
the diffusion welding parameters were: heating at 400 deg.C, holding for 90min, and welding under 10Mpa, and cooling the sample to below 100 deg.C to prevent oxidation of welded joint at high temperature.
Shear strength test: firstly, processing a diffusion welding joint into a sample with the thickness of 10mm multiplied by 20mm, assembling the diffusion welding sample on a special clamp by adopting a DNS200 type micro-control electronic universal test press and a special clamp, and testing the shear strength of the diffusion welding joint on a universal test machine, wherein the loading speed is 1 mm/min.
Before the shear test, the outer surface of the sample was ground flat to measure the shear area and to ensure the shear accuracy, and then the shear test was performed on a test press.
The shear strength of the brazed joint was 59KN/mm2(ii) a And (3) hardness testing: firstly, grinding a welding sample into two surfaces with high parallelism and certain smoothness by using water sand paper, and continuously grinding, polishing and corroding the surface with the hardness to be measured according to the requirements of a metallographic sample; then, performing microhardness measurement on different positions of the welding seam diffusion layer by adopting an HVS-1000A Vickers microhardness instrument; the hardness of the joint was 117 HV.
EXAMPLE six
Pretreatment in welding: roughly grinding a spreading test surface and a brazing surface of hard alloy and steel on a diamond grinding machine, then coating diamond grinding paste on an iron casting block, finally placing the spreading surface and the brazing surface on cast iron for grinding until the surfaces are bright, roughly grinding 45 steel on a grinding machine, then grinding the spreading test surface and the brazing surface to be bright by using metallographic abrasive paper, cutting the brazing filler metal CuMnTi into sheets, wherein the sizes of the brazing filler metal CuMnTi are slightly larger than the brazing surface so as to ensure that the brazing filler metal is enough to fill up brazing gaps, grinding the brazing filler metal and the iron sheets to be bright by using the metallographic abrasive paper, and removing an oxide layer;
soaking all polished materials in acetone for 5-10 minutes during brazing, scrubbing, taking out and drying; in order to prevent the sample from being polluted again, vacuum diffusion brazing needs to be carried out as soon as possible;
Plating Ni on the pretreated hard alloy, wherein the plating solution formula of the chemical nickel plating is as follows: 28g/L of nickel sulfate, 19g/L of sodium acetate, 17g/L of sodium citrate, 29g/L of sodium hypophosphite, 6-7 drops of thiourea and 30 drops of lactic acid, and adjusting the pH value to 4.5-5;
the alkaline washing liquid comprises the following formula: 20g/L of sodium hydroxide, 35g/L of trisodium phosphate, 25g/L of sodium carbonate and 2.5g/L of sodium silicate;
the plating process conditions are as follows: the alkali washing temperature is 60 ℃, and the alkali washing time is 10-15 min; after alkali washing, carrying out acid washing in hydrochloric acid for 10-15 s; the plating temperature is 80 ℃;
and (3) carrying out recrystallization annealing on the brazing filler metal: calculating and determining the lowest recrystallization temperature of the brazing filler metal according to an empirical formula, firstly closing a switch in a box-type resistance heating furnace, raising the furnace temperature to the annealing temperature, preserving heat for 60min, homogenizing the furnace temperature, then closing the resistance heating furnace, quickly opening a furnace door, feeding the brazing filler metal into the furnace, quickly closing the furnace door, closing the switch to continue heating, timing and preserving heat when the temperature reaches the annealing temperature, closing the switch after the test heat preservation time, cooling the furnace to the room temperature, taking out the brazing filler metal, coarsely grinding with No. 01 and No. 03 abrasive paper, finely grinding with No. 05 and No. 07 respectively after annealing, and then polishing on velvet by using A1203 polishing liquid until the surface is smooth and has no scratch;
Vacuum diffusion welding: in the test process, firstly, the processed hard alloy, steel and brazing filler metal are placed in a vacuum furnace, the hard alloy, the steel and the brazing filler metal are assembled, the furnace is vacuumized to 14Pa, parameters such as annealing temperature, heat preservation time, heating speed and the like are set on a controller, when the vacuum degree reaches 14Pa, pre-pressure is applied to 10MPa, the temperature starts to rise to a preset temperature at the speed of 22.5 ℃/min on average, and when the temperature rises to 200 ℃, the pressure is gradually increased due to the self expansion of the welding material.
The diffusion welding parameters are: heating at 400 deg.C for 70min, maintaining at welding pressure of 8Mpa, and cooling the sample to below 100 deg.C to prevent oxidation of the welded joint at high temperature.
And (3) shear strength test: firstly, processing a diffusion welding joint into a sample with the thickness of 10mm multiplied by 20mm, assembling the diffusion welding sample on a special clamp by adopting a DNS200 type micro-control electronic universal test press and a special clamp, and testing the shear strength of the diffusion welding joint on a universal test machine, wherein the loading speed is 1 mm/min.
Before the shear test, the outer surface of the sample was ground flat to measure the shear area and to ensure the shear accuracy, and then the shear test was performed on a test press.
The shear strength of the brazed joint is 55.76KN/mm2(ii) a And (3) testing hardness: firstly, grinding a welding sample into two surfaces with high parallelism and certain smoothness by using water sand paper, and continuously grinding, polishing and corroding the surface with the hardness to be measured according to the requirements of a metallographic sample; then, performing microhardness measurement on different positions of the welding seam diffusion layer by adopting an HVS-1000A Vickers microhardness instrument; the hardness of the joint was 115 HV.
According to the test results of the joint hardness of the embodiment, the invention utilizes the heating furnace to carry out recrystallization annealing treatment on the brazing filler metal, so that the matrix structure of the brazing filler metal is refined, and a good base material is provided for diffusion welding; when the hard alloy and the steel are welded, the physical and chemical properties of the hard alloy and the steel are different and influenced, so that the weldability of the hard alloy and the steel is poor, a large amount of intermetallic compounds with high brittleness and high hardness can be generated on a joint interface, and the performance of a welding joint is seriously influenced; by plating Ni on the hard alloy, the generation of intermetallic compounds is avoided or reduced, the types and the distribution states of the intermetallic compounds generated at the joint are improved, the strength of the joint is improved, and meanwhile, vacuum diffusion welding is adopted to weld dissimilar metals of the hard alloy and steel, so that the welding quality with better quality can be obtained.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.

Claims (3)

1. A vacuum diffusion welding process of hard alloy and steel is characterized in that: the method comprises the following steps:
pre-welding treatment: roughly grinding a spreading test surface and a brazing surface of hard alloy and 45 steel on a diamond grinding machine, then coating diamond grinding paste on an iron casting block, and placing the spreading test surface and the brazing surface on cast iron for grinding until the surfaces are bright; polishing the spreading test surface and the brazing surface by using metallographic abrasive paper; polishing the brazing filler metal by using metallographic abrasive paper to be bright, and removing an oxide layer;
soaking all polished materials in acetone for 5-10 minutes during brazing, scrubbing, taking out and drying;
plating Ni on the pretreated hard alloy, wherein the plating process conditions are as follows: the alkali washing temperature is 60 ℃, and the alkali washing time is 10-15 min; after alkali washing, carrying out acid washing in hydrochloric acid for 10-15 s; the plating temperature is 80 ℃;
Carrying out recrystallization annealing on the brazing filler metal;
vacuum diffusion welding: firstly, placing the treated hard alloy and 45 steel into a vacuum furnace, assembling the hard alloy, 45 steel and brazing filler metal, vacuumizing the furnace to 14Pa, applying a pre-pressure of 10MPa when the vacuum degree reaches 14Pa, starting to heat up to 200 ℃ at a speed of 22.5 ℃/min, and then starting to heat up to 500 ℃ at a speed of 25 ℃/min; keeping the heating temperature between 400 and 500 ℃ during diffusion welding, keeping the temperature for 60-180min, and the welding pressure at 0-10Mpa, and cooling to below 100 ℃ along with the furnace after the welding is finished;
the brazing filler metal is CuMnNi or CuMnTi or iron sheet.
2. The vacuum diffusion welding process of cemented carbide and steel according to claim 1, characterized in that: the formula of the plating solution for chemical nickel plating is as follows: 28g/L of nickel sulfate, 19g/L of sodium acetate, 17g/L of sodium citrate, 29g/L of sodium hypophosphite, 6-7 drops of thiourea and 30 drops of lactic acid, and adjusting the pH value to 4.5-5; the alkaline washing liquid comprises the following formula: 20g/L of sodium hydroxide, 35g/L of trisodium phosphate, 25g/L of sodium carbonate and 2.5g/L of sodium silicate.
3. The vacuum diffusion welding process of cemented carbide and steel according to claim 1, characterized in that: the recrystallization annealing treatment specifically comprises the following steps:
firstly, a box type resistance heating furnace is subjected to empty furnace heating and heat preservation for 60min to homogenize the furnace temperature, then the box type resistance heating furnace is closed, the furnace door is quickly opened to send brazing filler metal into the furnace, the furnace door is quickly closed, the box type resistance heating furnace is opened to continue heating, heat preservation treatment is carried out when the temperature reaches the annealing temperature, natural cooling is carried out after the heat preservation treatment, after annealing, No. 01 and No. 03 abrasive paper are used for rough grinding, No. 05 and No. 07 fine grinding are respectively used for fine grinding, and then A1203 polishing solution is used for polishing velvet until the surface is smooth and has no scratch.
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